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Evaluation of New Applications of Oil Shale Ashes in Building Materials

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Evaluation of New Applications of Oil Shale Ashes in Building Materials minerals Article Evaluation of New Applications of Oil Shale Ashes in Building Materials Mustafa Cem Usta 1,*, Can Rüstü Yörük 1, Tiina Hain 2, Peeter Paaver 3, Ruben Snellings 4, Eduard Rozov 5, Andre Gregor 1, Rein Kuusik 1, Andres Trikkel 1 and Mai Uibu 1 1 Department of Materials and Environmental Technology, Tallinn University of Technology, 19086 Tallinn, Estonia; [email protected] (C.R.Y.); [email protected] (A.G.); [email protected] (R.K.); [email protected] (A.T.); [email protected] (M.U.) 2 Department of Civil Engineering and Architecture, Tallinn University of Technology, 19086 Tallinn, Estonia; [email protected] 3 Department of Geology, University of Tartu, 50411 Tartu, Estonia; [email protected] 4 Sustainable Materials, VITO, 2400 Mol, Belgium; [email protected] 5 Wienerberger, 43401 Aseri, Lääne-Virumaa, Estonia; [email protected] * Correspondence: [email protected] Received: 3 July 2020; Accepted: 27 August 2020; Published: 29 August 2020 Abstract: Achieving sustainable zero-waste and carbon neutral solutions that contribute to a circular economy is critically important for the long-term prosperity and continuity of traditional carbon-based energy industries. The Estonian oil shale (OS) sector is an example where such solutions are more than welcome. The combustion of OS generates a continuous flow of ashes destined to landfills. In this study, the technical feasibility of producing monolith building materials incorporating different OS ashes from Estonia was evaluated. Three binder systems were studied: self-cementation of the ashes, ceramic sintering in clay brick production and accelerated carbonation of OS ash (OSA) compacts. Results showed that most of the OSAs studied have low self-cementitious properties and these properties were affected by ash fineness and mineralogical composition. In case of clay bricks, OSA addition resulted in a higher porosity and improved insulation properties. The carbonated OSA compacts showed promising compressive strength. Accelerated carbonation of compacted samples was found to be the most promising way for the future utilization of OSAs as sustainable zero-waste and carbon neutral solution. Keywords: oil shale ash; waste utilization; concrete; bricks; carbonation curing 1. Introduction New initiatives by the European Commission not only aim at reducing air and water emissions but also extensively encourage innovation in waste or residue recovery using “Best-Available Technologies” (BAT) that promote transitions towards green energy production under the principles of circular economy [1]. In this context, the Estonian oil shale (OS) sector is a good example where the management and utilization of waste is vital to ensure long term sustainability. Estonia is still mostly utilizing low calorific fuel—OS as a primary source of energy including electricity, heat and oil production across the country. This heavy fossil fuel reliance produces abundant amounts of uncommon calcareous ash which has been deposited in landfills and waste piles over the years, since the ash lacks industrial applications [2,3]. Historically landfilled ashes as well as the currently generated ashes carry important risks to the biosphere such as emissions of hazardous trace elements (Sr, Zr, As, Cd, Cu, Cr, Zn, Pb) as well as alkalinity to groundwater and air [4–6]. In recent decades the implementation of circulating fluidized bed (CFB) boilers for combustion and advanced retorting technologies for oil production have greatly increased extraction efficiencies Minerals 2020, 10, 765; doi:10.3390/min10090765 www.mdpi.com/journal/minerals Minerals 2020, 10, 765 2 of 19 and reduced GHG emissions. However, these changes in the process are not without pitfalls as the physical and chemical characteristics of the OSA were negatively affected. For instance, lowering the temperatures from 1300–1400 ◦C (previously used in pulverized firing (PF) boilers) to 700–800 ◦C (used in current CFB boilers) changed the phase composition of the ashes, altered the content of unburnt materials and increased calcium sulfate contents. The phase composition shifted away from high-temperature Ca-silicates towards free lime and quartz. This complicates the utilization of OSA by inducing volumetric expansion and poses environmental issues by increasing the pH of OSAs [7]. The utilization of OSA in the production of new valuable products could be a partial solution for the Estonian OS sector by integrating core concepts from circular economy. In this respect, OSA as any other industrial alkaline solid waste (such as lignite, coal, wood bottom and fly ashes (FAs), steel slags, cement production wastes and waste concrete), can be considered as a valuable raw material in the conventional production processes of cement, concrete and ceramics [8–10]. Evidence of this utilization has existed previously in the Estonian context, where OSA, collected from electrostatic precipitators (EP) of PF units, was used as a raw material for the production of Portland clinker. Additionally, coarse fractions were used as aggregates in the production of cellular concrete blocks and in the applications of road-base stabilization [2,7]. However, due to the above-mentioned changes in the OS incineration process such applications have been phased out. Therefore, there is an urgent need to investigate alternative application routes for OSAs. The current study includes three sub-studies of oil shale ash utilization in building materials; first sub-study is testing of self-cementing properties of all the currently generated OSAs, second sub-study is the clay brick production with oil shale ash to test its performance as opening agent and the last sub-study is on the properties of OSA monoliths obtained by accelerated carbonation, which draws on the recent developments in research of carbonate bonded construction materials [11–13]. 2. Materials and Methods 2.1. Self-Cementing Performance 2.1.1. Materials A range of OSAs were included in the present study. The selected ashes were mainly FAs regularly collected in the period of 2018 and 2019 including electrostatic precipitator ash (EPA), cyclone ash (CA), total ash (Mixture of all flow of ashes from PP, except EPAs) (TA) and mixtures of different FAs from the Auvere (A) and Eesti (E) power plants (PP). Additionally, CA and TA from the Enefit 280 oil production plant were included. In total, 6 different ash streams (EPP-EPA, EPP-TA, APP-EPA, APP-TA, EN280-CA, EN280-TA) were considered. 2.1.2. Material Characterization The physical, chemical and mineralogical characterization of the selected waste streams included determination of total carbon (TC) and total inorganic carbon (TIC) with an Eltra CS 580 (Haan, North Rhine-Westphalia, Germany) Carbon Sulphur Determinator and free CaO content (based on ethylene glycol method), X-ray fluorescence (XRF) and X-ray diffraction (XRD) analyses with Bruker S4 Pioneer (Karlsruhe, Baden-Württemberg, Germany) and Bruker D8 (Karlsruhe, Baden-Württemberg, Germany) diffractometers, respectively. For XRD analysis, randomly oriented preparations were made and scanned on a Bruker D8 Advance diffractometer using Cu Kα radiation with a Göbel mirror monochromator and LynxEye positive sensitive detector over a 2◦–70◦ 2Q range. The quantitative phase composition was analysed and modelled using the Rietveld algorithm-based program Topas (Karlsruhe, Baden-Württemberg, Germany). The relative error of quantification is better than 10% for major phases (>5 wt. %) and better than 20% for minor phases (<5 wt. %). The BET-N2 sorption method was used to measure the specific surface area (SSA) with Kelvin 1042 sorptiometer. Minerals 2020, 10, 765 3 of 19 The particle size distribution (PSD) was measured by laser diffraction using a Horiba (Kyoto, Japan) Laser Scattering instrument, LA-950 (with ethanol suspension). 2.1.3. Sample Preparation In order to test the self-cementing properties of the OSAs, ash and sand pastes were prepared for all waste streams. 0.7 was found to be optimum ratio of water to ash [14] and ash to sand (cf. EN 196-1:2016) ratio was 0.33. Pastes were cast in 40 40 160 mm3 prisms and compacted using × × a vibration table. The compacted pastes were first kept 48 h in molds, then five days at 60% RH and 20 2 C, and further curing continued for 28 days at >95% RH and 20 2 C. After 28 days, ± ◦ ± ◦ the failure strength (flexural and compressive strength) was tested following EN 196-1:2016 [15]. The aim of the work regarding self-cementing properties of oil shale ashes was to find possibilities for utilization of oil shale ashes. These types of studies are based on our own experience with oil shale throughout the years. The methods described therein might vary from those utilized in the applications of Portland cements due to the distinct influence of OSA types and properties of pastes and mortars. 2.1.4. Tests and Measurements Flexural strength test determined the maximum bending stress of prisms before failure. This test was conducted on a Toni TechnikD-13355 (Berlin, Brandenburg, Germany) which works in accordance with EN ISO 7500-1 (2018) [16]. The compressive strength test was also performed using the same apparatus which applies a progressing load rate of 2400 N/S in accordance with EN 196-1:2016 and ISO 679 [17]. The split mortar bar halves from flexural strength test were used for the compressive strength measurements. 2.2. Clay Bricks with Sand to OSA Replacement 2.2.1. Materials The clay (Cambrian blue clay) and clay/sand mixtures used in the green shaped bodies were obtained from Wienerberger Company—located in Aseri, Estonia. Similar physical and chemical characterization methods, as defined above for concrete application, have been used for the material characterization of the clay. The studied OSA sample for clay bricks is EPP-EPA obtained in August 2018 which was separated into different size fractions by size classification. The coarse fraction was used as sand or opening agent replacement in the formulation of clay bricks. Material characterization considered both the initial EPP-EPA and coarse fraction of EPP-EPA in terms of PSD, SSA, XRF and XRD analyses.
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